Method of and apparatus for separating sulfur from sulfur ores



N. E. KATZ.

METHOD OF AND APPARATUS FOR SEPAHATING SULFUR FROM SULFUR DRES- APPLICATHJN FILED JUNE 24. I919.

1,365,922, Pa-tented Jan. 18, 1921.

UNITED STATES PTENT OFFICE.

NAHUM E. KATZ, OF MERIDIAN, MISSISSIPPI, ASSIGNOR OF ONE-HALF TO HORACE M. LITTLE, OF ll/IEEIDIAN, MISSISSIPPI.

METHOD OF AND APPARATUS FOR SEPARATING SULFUR FROIVI SULFUR OBES.

Application filed June 24, 1919.

To all whom it may concern:

Be it known that I, NAHUM E. Ka'rz, a citizen of the United States, residing at Meridian, in the county of Lauderdale and State of Mississippi, have invented certain new and useful Improvements in Methods of and Apparatus for Separating Sulfur from Sulfur Ores, of which the following is aspccification. I

My invention relates to a method and apparatus for separating sulfur from sulfur ores and is based on the discovery that if sulfur ore is heated in an autoclave or digester, in the presence of steam, at suitable pressure, the sulfur is quickly and completely extracted in a highly refined condition under more economical conditions than have heretofore been used. The use of an autoclave particularly of the construction hereinafter described results in economies in operation and of heat consumption which are not obtained by the ordina-ry'methods.

I am aware that it has been proposed to extract sulfur from its ores by subjecting it to the action of steam in a closed vessel, but these prior processes have disadvantages which are overcome by my present invention.

The apparatus is shown, more or less diagrammatically in the accompanying drawings, but sufliciently to indicate the principles of operation.

In the draw ings,-

Figure 1 is a vertical section of the apparatus;

Fig. 2 is a vertical section of a modification of the ore containers;

Fig. 3 is a vertical section of a modification of the autoclave or digester; and

Fig. l is a cross section of a. modified form of basket.

In Fig. 1, X is an autoclave built sufficiently strong to withstand high steam pressures. In the bottom ofthis autoclave is placed a certain amount of water, the level of which is indicated by the gage 9. This water level may be maintained -con stant by any known automatic or other device. Any suitable means for heating the autoclave may be used, and I have indicated a gas burner 7 as located beneath the autoclave. 2 is a tight fitting cover which is held in place by a series of bolts 3 with wing nuts, or by clamps. or in any other well known manner. 4: is a conduit con- Specification of Letters Patent.

Patented Jan. 18, 1921.

Serial No. 306,385.

nected to the cover and provided with a safety valve 40 and a pressure gage 10. 5 is a valved pipe for permitting the escape of the air in the autoclave when displaced by the steam generated therein.

Supported in the autoclave by any suitable means and near the bottom thereof is a pan A into which runs all the sulfur that is eX- tracted from the ore. On top of the pan A may be placed a cover made of filter cloth, so that themolten sulfur may be further purified before it reaches the pan A. The bottom of the pan may be either horizontal or slightly inclined toward the outlet 0 which is provided with a valve E regulated by a handle F on the outside of the autoclave. TheeXit pipe H connected with the outlet 0 terminates outside the autoclave.

.Mounted within the autoclave are a series of baskets B placed one on top of the other, these baskets being filled with the ore from which the sulfur is to be extracted. The baskets'may be introduced into the autoclave or withdrawn from it either separately or in group. The baskets B have perforated bottoms and secured thereto are inclined conical plates of slightly larger diameter than that of the bottom.

The baskets may be constructed in accordance with the modification shown in Fig. 2 in which each basket is provided with a central conduit 15, and beneath each basket is arranged a conical funnel shaped plate 16 for delivering the molten sulfur down through the conduits. 1

In either form of basket shown the molten sulfur as it is melted out of the ore flows ontothe plates and is delivered into the pan A. The bottoms of the baskets may bemade removable and may be corrugated as well as perforated; or they may be corrugated or covered with metal cloth or flat perforated metal, as shown in Fig. 4.

The mode of operation is as follows. A proper amount of water is placed in the bottom of the autoclave and the baskets B filled with the ore from which the sulfur is to be extracted are then introduced into the autoclave. The top 2 is then secured in place by means of the bolts 3 so that a steam tight closure is effected. The valve 5 is then opened and the valves E and 8 are tightly closed. The Water in the bottom of the autoclave is then heated sufficiently to generate steam. .As soon as the operation repeated.

air in the autoclave is displaced by the steam, as will be shown by the escape of steam from the valve 5, the valve 5 is closed and the heating continued. The steam within the autoclave now begins to rise in pressure and temperature, and as soon as the desired steam pressure has been reached, the supply of gas to the burner 7 is cut down to just a sulticient volume to maintain the steam pressure constant for the desired length of time. After the steam has acted on the ore for some time and some sulfur has been collected in the pan A, the valve E is gradually opened and the liquid sulfur which has collected in the pan A begins to run out. The valve E is then kept open until all the sulfur has been extracted and the process is completed.

WV hen the extraction is finished the heating of the autoclave is discontinued and the valve 8 gradually opened and the steam blown out either into the open air or into another autoclave. If several autoclaves are operated together the steam escaping through the valve 8 is conducted into another autoclave which has just been prepared ready to start an operation. hen the pressure in both autoclaves has equalized itself they are disconnected and the balance of the steam in the autoclave which has just finished operation is either allowed to escape into the air or is utilized to preheat the water which is to be introduced into the autoclaves.

When the pressure in the autoclave o1 digester has fallen to zero, the top is removed and the series of baskets containing the residual ore is taken out to be emptied. Another series of baskets is filled with fresh ore, introduced into the autoclave, and the The particular pressures to be used have not been specified but such temperatures must be employed as will be sufficient to raise the temperature of the sulfur within the ore above its melting point, which is about 115.

My improved method obviates the necessity of having a boiler plant for the generation of the steam required, which is generated within the autoclave itself and is thus obtained at a considerable saving of fuel. Each autoclave is thus an independent unit and a complete and economical plant irrespectiv'e of its size or capacity. Furthermore, this apparatus is suitable for field use and can easily be installed anywhere and in any desired locality.

My method of application of steam also has other advantages. Thus, if the steam is carried into the extraction vessel from an outside boiler as has heretofore been the practice, there is undue condensation and consequent loss of heat. This condensation not only interferes with the extraction process but necessitates the use'of large volumes of steam to supply the required amount of heat. It is further the practice, in order to maintain a constant pressure within the extraction vessel to permit a portion of the steam to escape into the air during the time operation is going on, thus considerably increasing the cost of the process.

Further difficulties ensue from the condensation of steam since the condensed. water permeates the extracted sulfur and makes the residual ore wet and difficult to handle when it is removed from the extractor.

By my improved process, only such volumes of steam are required as suffice to fill the vacant space in the autoclave, and I have found that the sulfur comes out dry and that the residual ore when removed from the autoclave is also perfectly dry and brittle.

The use of a series of baskets or ore containers has the particular advantage that the ore to be extracted is not contained in a large solid bulky mass but is subdivided into a number of rather shallow masses, thus exposing to the action of the steamheat a very large ore surface, and the sulfur extracted from each basket is not compelled to pass through any other masses of ore to reach the collecting pan. The formation of pools of sulfur within the body of the ore is thus avoided and complete extraction of the sulfur is assured, while at the same time the cementing together of the gangue when the process is finished is prevented.

A further advantageous modification of the form of the autoclave is shown diagram matically in Fig. 3. In this form of appa ratus the water from which the steam is generated instead of being placed in the bottom of the autoclave is contained within a vessel W communicating with the autoclave by means of a pipe P having a valve V. I have observed that in the ordinary autoclave as shown in Fig. 1 when the steam pressure has gone down to zero there is still evolution of steam from the water which is practically at boiling point. This steam interferes with the emptying and filling of the autoclave which causes a waste of time. Furthermore, the heat supply being shut off the temperature of the water falls considerably below the boiling point before the autoclave is ready to start into operation. These advantages are eliminated by the construction shown in Fig. 3. When the extraction is complete the heat supply need not be cut off, but the valve V is tightly shut, thus stopping all steam supply to the autoclave to permit the continued heating of the water within the vessel W. WVhe'n the autoclave is again ready for operation the valve V is opened and the steam supply is immediately available.

While I have shown an upright form of autoclave, it is obvious that the autoclave may be horizontal and in such case the has kets or ore containers may be placed on trucks provided with wheels so that the trucks with the ore may be conveniently introduced into the autoclave and removed therefrom. Obviously also the autoclave may be properly heat insulated in a brick or other setting to permit utilization to good advantage of the combustion gas, in any well known manner.

My invention is not limited to any specified number of baskets, nor to their shape, form or size, nor to the shape, form or size of the perforations.

I claim:

1. The method of recovering sulfur from sulfur ores containing the same, which consists in heating the ore in an autoclave in the presence of water to a temperature sufli cient to melt the sulfur by means of steam generated in said autoclave.

2. The method of recovering sulfur from ores containing the same, which consists in heating-subdivided masses of the ore in an autoclave in the presence of water to a temperature sufiicient to melt the sulfur by means of steam generated in said autoclave.

8. The method of recovering sulfur from ores containing the same, which consists in heating subdivided masses of the ore in an autoclave in the presence of water to a temperature sufiicient to melt the sulfur by means of steam generated in said autoclave, and collecting the sulfur separately from each such mass.

In testimony whereof, I afiix my signature.

NAHUM E. KATZ. 

